Glycerin-still.



PATBNTED MAR-20, 1906. k

' GJSUDRE. LYGBRIN STIL OATION FILED mac W (T N 5.55 s. s

ATTO R N aYs pfiled by me'on as possible.

PATENT O ICE.

CHARLES- 'SUDRE, o F PARIS, FRANCE.

GLYCEFtlN-STIL L.

I Application filed DecemharIBO, 1902. $erial No. 137,127.

Specification of Letters Patent.

Patented March 20, 1906.

To all, whom it may concern: j Be it known that I, CHARLES SU RE,residing at 33 Boulevard Haussmann, Paris, in the Republic of France,have invented a certain new and useful Glycerin-Still and I do herebydeclare the following to be a full, clear, and exact descriptionof theinvention, suchas will enable others skilled in the art to which itappertains' to make and use the same. A divisional application of thiscase was January 6, 1904, Serial No. 187,931. Up 7 to the present in anyapparatus or rocess for treating the residuary liquors rom alcoholdistillation in order to extract from them glycerin andother usefulproducts some mechanical apparatus forscraping or; cleaning theexhausted products has always had to be employed. By reason of the very;construction of anyprevious apparatus numerous accompaniments areproduced which pass into the distilled liquid and render it very;

impure. It is well known that in order tof extract the glycerin withoutdecompositionit is necessary to work in as complete a vacuum;

ter and a little glycerin, when, the material duces a froth andcarriesfnumerous particles, which hinder the operations and in many offthe processes used up to now render the working impossible if the dregsare viscous.

The apparatus which is the subject*of=the present application for apatent does away with this inconvenience. It is based on the followingdiscoveries and appliances:

First. :If the vinasse' from a distillery (of "treacle,'for example) bedistilled in a vacuum at a temperature of not' more'than 300, the

'residue after the-glycerin and the water have been "extractedisliquidat this temperature of "300 "and fiows away of its ownaccord. Theglycerin and water are extracted in'a' time which depends onthethickness of the vinassaQ-My processconsists-in rinciple of providingalong the walls of-an inc osure suit- "abl garranged," in which'there isa'vacuum an which is heatedfb some exterior source of heat in -such awaythat the temperature of 'thewalls "cannot-be greater than 300, aconstant stream of :itli' 'vin asse' 'of regular and 5 5 regulatedthickness: "Thus the vinasse 'en' The vinasse under the action of heatand in a vacuumfirst of all distilswa tersand pours awayin a continuousliquid state without. the intervention, of any me chanical apparatus andloses in its passage (supposingthat thisis of a lengthsuitable to thethickness of the liquid film) first of all its water and then itsglycerin. t

Second. It is proved that if the vinasse is sufficiently acidulated theammonia only escapes in infinitesimal proportions and remainsconcentrated in the'residue.

Third. By forcing the vapors to take up in the apparatus itself a rapidgyratory helicoidal movement I obtain by centrifugal force theimpingement against the heated walls of the particles carried by thevapors, which distil anew;

Fourth. It isadmitted that it is necessary to have a current ofsuperheated steam to help the distillation of the glycerin when thevinasse has become anhydrous.

v processes this steam is introduced from without, and thus dilutes thecondensed mixture of water and glycerin. I utilize for this purpose thesteam arising from the vinasse itself, which is superheated in theapparatus while taking up its gyratory .movement. The superheated steamthen bathes and surrounds before'it leaves the apparatus the glycerin,which is given off by the anhydrous substance and draws it out of 1These principles being setforth, I will describe as'a representativeexample a construction for the carrying out of the process shownins'ection diagramatically in the accompanying drawing'and by which Iput. these'princlplesxinto' practice but it is evi dent that'the formsmay be infinitelyvaried.

"The apparatus is designed to be heated by too 1 coke or charcoal. I Itconsists of a distillingcolumn a,'formed of flangedcast ron tubes, threetosix meters high, according to the quantity of "water in the vinasse tobetreated; Above this column is situated a 105 distributer. 1, whichspreads throu han an} nular passage onto the interior wa ls of the'columna' continuous stream of the vinasse to-be treated; At the footofthis column is placed a pipe 2 for the escape of the gas and no In manyOn the contrary,

vaporswhich are given off by the vinasse under treatment. Below this thecolumn is constricted and is terminated by a chamber 1), provided withstop-cocks c and d and in which the residue collects and which isarranged in such a Way that it can be drained off at regular intervals.Inside the column a is suspendedor fastened in any convenient way a rodf, round which'is coiled a helix 9, of which the outside surface is veryclose to the walls of the cast-iron column. The gas 7 and vapors escapeinto a shorter accessory column h, called the purifying-column, smallerthan the principal column, but also containing a fixed helix. The solidsubstances drawn in impinge onto the walls and, distilling glycerinwhile descending the whole 7 length of the walls, enter a chamber likethe V first, while the gas and purified vapor are directed into acondenser i by a suction-pump 7c. The whole is inclosed within a casingof V refractory material m, leaving sufficient space between it and thecolumn for the passage of the gases for heating the apparatus. Thesegases are produced in a furnace n, placed outside the column. Thisfurnace is fed by coke .or charcoal and is supplied with air by a blower0. The hot gases proceed by a vertical flue p to the top of the casinginclosing the column. In their passage a second blower q injects coldair into them in a regulated quantity, so that their temperature at thetop of the column is from 600 to 700 centigrade. Thegases redescend incontact with the cast-iron column and produce the evaporation of thewater, whereby the greater portion of their heat is abstracted- Aboutthe middle of the column the gases are not more than 300. The smallcolumn h annexed. should not be higher than this point. As from otherreasons the distillation of the rest of the glycerin, which is in verysmall quantities, requires very little heat, the temperature remainspractically the same till it escapes by the lower flue.

The vinasse being watery and admitted to the vacuum, the Water containedis distilled at and in consequence until all the water is distilled thetemperature of the vinasse scarcely rises above this in spite of thegases outside being at a temperature of 600 or .7.00 centigrade, all theheat of these being 7 used up to distil the water.

condenser connected. to said The steam produced. inside and at the topof the column exhausted by the suctionpump is required to descend, whichit does by following the path of the helix, taking up a gyratorymovement, which by the centrifugal force developed rids it of all theparticles which are thrown against the wall, where the distillation iscompleted. While descending, the steam becomes superheated and helps inthe distillation of the glycerin in the anhydrous portions.

Let us now follow an operation: The vinasse previously concentrated hassome acid added to it, so as to corres 0nd to four or five per cent. ofH SO T ien it is introduced into the top of the column, which has firstof all been brought to the proper temperature by heating. The vinassespreads in a film and submitted to heat in a vacuum undergoes a violentebullition. It descends the length of the walls and loses first of all,as has been explained, its water and then. becoming superheated, itsglycerin. The steam in the upper portion, which contains particles insuspension, enters the interior helix. The particles und er the actionof centrifugal force are projected against the wall and furtherdistilled and becoming heated surround and draw the escaped glycerinfirst into the accessory column h, Where it undergoes a freshpurification, then into the condenser, where it becomes liquid. Thereslduary gases after havmg been drawn through the suction-pump arewashed to rid them of any nitrogenous material they may contain, andthen they escape into the at- V mosphere. The substances deposited inthe accessory column undergo, as I have already described, a freshdistillation and the glycerin they distil merges into the glycerin-vaporfrom the principal column, which vapor passes through the accessorycolumn. The

. substances deprived of glycerin flow into the bottom chamber, fromwhence by means of successive movements of the sto -cocks they arewithdrawn at intervals. hus by this a paratus is obtained, first, amixture of g ycerin and water of great purity, which has only to beconcentrated to obtain glycerin ready for sale; second, a residuaryliquid,

very hygrometric, which solidifies in air, retaining all potash andnitrogen, which can be sold as it is for manure or be redistillcd withlime to produce ammonia, methylamin, pyridic tars, or be treated in anyother suitable manner.

I claim 1'. An apparatus for the purpose described comprising a verticalcolumn, a stationary internal helix therein, a connected purifyin columnat the side, a stationary helix in sald purifying-column, and asuction-pump and purifying-column, substantially as described.

2. An apparatus for the purpose described comprising a verticalcolumnhaving a cham- In testimony whereof I have hereunto set ber atthebottom, a stationar internal helix my hand in the presence of twosubscribing Io therein,asinallerpuiifying-co grnn afi the Sid?Witnesses. i

havin its ower en connecte to t e to 0 5 the fil st column, a stationaryhelix in Said CHARLES S I purifying-column, and a suctionump andWitnesses: condenser connected to said unfying-col v ANDRE MOSTIOKER,umn, substantiallyas described EDWARD P. MAQLEAN.

